CN108499373A - A kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material - Google Patents
A kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material Download PDFInfo
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- CN108499373A CN108499373A CN201810310498.XA CN201810310498A CN108499373A CN 108499373 A CN108499373 A CN 108499373A CN 201810310498 A CN201810310498 A CN 201810310498A CN 108499373 A CN108499373 A CN 108499373A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The present invention relates to a kind of preparation methods of super hydrophilic oleophobic type film base water-oil separating material, belong to oily water separation technique field.The present invention is using chitosan and nano-titanium dioxide as water wetted material, the film with fish scale surface micro emulsion lug structure is prepared by template, it is reacted simultaneously using ammonia and carboxylic acid ion present in nano titanic oxide sol, generate ammonium salt, polar water can interact with ammonium salt, the hydrophilic radical of film coated surface is set to migrate, and chemisorption water layer can be formed by ultraviolet light-initiated smooth nano-titanium dioxide surface, as hydrophilic layer, recycle the polycondensation reaction of hydroxyl silicon, with the hydroxyl group that chitosan surface is abundant, the silicon oxide particle formed for solution provides fixed point, and the common cetrimonium silane that polycondensation reaction occurs provides long alkyl chain for the silicon oxide particle formed, make film surface that there is lower surface energy, there can be special wetting property.
Description
Technical field
The present invention relates to a kind of preparation methods of super hydrophilic oleophobic type film base water-oil separating material, belong to oily water separation technique
Field.
Background technology
With the rapid development of economy, the discharge of all kinds of oil spill accidents and oily wastewater causes water body and ecological environment
Oil pollution be consequently increased, to also gradually being aggravated to the injury that the mankind bring.In order to protect the ecology in China and the world
Environment, prevention oil pollution, the preparation and application study for carrying out efficient oil absorption material and water-oil separationg film have important scientific research
Value and realistic meaning.Excellent oil absorption material should have super-hydrophobic super-oleophylic characteristic, higher oil absorption, good oil storage
The features such as easily being recycled after effect, oil suction, while there are the performances such as good reuse and biodegradability；Film base water-oil separating
Material should more have efficient water-oil separating characteristic.But current existing oil absorption material is in oil absorption, material reuse and oil
All there is disadvantage in water seperation film, which has limited their practical applications in oil-water separation etc..
China generates 5,000,000,000 tons of oil field extracted waters every year, if can be efficiently separated grease using effective technology, can not only incite somebody to action
Oil-field flooding recycles, using water wisely, moreover it is possible to improve oil recovery amount；Although major part water-oil separating material can be by greasy dirt at present
Separation or adsorbing and removing from oil water mixture, but this kind of material is easily blocked by greasy dirt, access times and using effect by
Larger limitation；In addition, another water removing class material can selectively remove the water in oil water mixture, and can be effectively
Avoid absorption and blocking of the membrane material to oils, but need complicated chemical modification step in its preparation process, and its
State labile in complicated oil pollution environment.Membrane material for water-oil separating is referred to as film base water-oil separating material,
Water-oil separationg film is may be simply referred to as, can be divided into inoranic membrane and organic polymer films two major classes, inoranic membrane has high temperature resistant, strong acid, strong
The advantages that alkali, organic solvent and resistance to microbial attack, high mechanical strength, narrow pore-size distribution, but there is also filming technology complexity
The poor reproducibility of (calcination), film, preparation small-bore film are difficult, poor, of high cost, the manufactured component of the crisp flexibility of matter assembles difficulty etc.
Disadvantage；Organic film preparation process is simple, and membrane material is wide in variety, is easy to be modified, flexibility is good, cheap, can be made into various shapes
The membrane module of formula, but organic film has pore-size distribution wide, and mechanical strength is low, and permeability is low, is easy hydrolysis, the resistance to temperature difference, and pH value is fitted
The shortcomings of with narrow range.Therefore, the application study that high efficiency oil-water separation material carries out the water body of pollution water-oil separating is prepared, tool
There are major and immediate significance and scientific research value.
Invention content
The technical problems to be solved by the invention：For the interface imbibition characteristic unobvious of current water-oil separating material, easily
The problem of being blocked by greasy dirt, causing access times with using effect by larger limitation, provides a kind of super hydrophilic oleophobic type film
The preparation method of base water-oil separating material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Natural air drying after black carp scales are washed with deionized 2~3 times, then it is used in combination 502 glue viscous at plate fish scale linking
Form type, obtains template base material；
（2）Ethyl orthosilicate, hexadecane trimethoxy silane is taken to be added in isopropanol and be uniformly mixed, then mass fraction is added dropwise and is
20% hydrochloric acid stirs 20~30min, obtains Ludox；
（3）It is that stirring to chitosan is completely dissolved in 2% acetum, then four fourth of metatitanic acid is added dropwise to take chitosan that mass fraction is added
Ester stirs 20~30min, obtains coating liquid；
（4）Coating liquid is coated on template base material surface, is placed in hydro-thermal process in hydrothermal reaction kettle, alcohol washes drying after reaction
And film is taken off, then film layer is immersed in Ludox and is stirred to react 3~5h, drying after film layer is washed with alcohol wash water successively is taken out, is obtained super
Hydrophilic and oleophobic type film base water-oil separating material.
Step（2）The ethyl orthosilicate, hexadecane trimethoxy silane, isopropanol, hydrochloric acid parts by weight be 8~12 parts
Ethyl orthosilicate, 1.0~1.5 parts of hexadecane trimethoxy silanes, 100~150 parts of isopropanols, 2~3 parts of hydrochloric acid.
Step（3）The chitosan, acetum, butyl titanate parts by weight be 2~3 parts of chitosans, 200~300
Part acetum, 4~6 parts of butyl titanates.
Step（4）The film amount of the coating liquid is 60~80g/m2。
Step（4）The hydrothermal treatment process is that 10~12h is reacted under 120~160 DEG C of ammonia atmosphere.
Step（4）It is described to be stirred to react to adjust pH to 9~10 with ammonium hydroxide and stirring 3~5h with 400~500r/min.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is prepared micro- with fish scale surface using chitosan and nano-titanium dioxide as water wetted material by template
The film of mastoid process structure, while being reacted using ammonia and carboxylic acid ion present in nano titanic oxide sol, it generates
Ammonium salt, polar water can interact with ammonium salt, and the hydrophilic radical of film coated surface is made to migrate, and nonpolar oils
Hydrophilic radical cannot be made to migrate, and chemisorption water layer can be formed by ultraviolet light-initiated smooth nano-titanium dioxide surface,
As hydrophilic layer, the polycondensation reaction of hydroxyl silicon is recycled, with the hydroxyl group that chitosan surface is abundant, the oxidation formed for solution
Silicon particle provides fixed point, and the common cetrimonium silane that polycondensation reaction occurs provides for the silicon oxide particle formed
Long alkyl chain makes film surface have lower surface energy, can have special wetting property；
（2）Water-oil separating material prepared by the present invention has good underwater hydrophilic and oleophobic performance, and anti-stick antifouling property is good, can be with
Good for water-oil separating durability, oily contact angle can reach 158 ° or more, and the present invention's is simple for process, can Mass production,
It is at low cost, use easy to spread.
Specific implementation mode
Natural air drying after black carp scales are washed with deionized 2~3 times, then fish scale is spliced into plate, it is used in combination 502 glue viscous
Form type, obtain template base material, takes 8~12g ethyl orthosilicates, 1.0~1.5g hexadecane trimethoxy silanes, it is added 100~
In 150g isopropanols, 20~30min is stirred with 300~400r/min, then 2~3g mass fractions are added dropwise with 0.1~0.2g/min
For 20% hydrochloric acid, continue 20~30min of stirring, obtain Ludox, take 2~3g chitosans, it is 2% that 200~300g mass fractions, which are added,
It in acetum, is stirred to chitosan and is completely dissolved with 300~400r/min, then 4~6g metatitanic acids are added dropwise with 0.3~0.5g/min
Four butyl esters continue 20~30min of stirring, obtain coating liquid, template base material surface coat coating liquid, control film amount be 60~
80g/m2, it is placed in hydrothermal reaction kettle, 10~12h is reacted under 120~160 DEG C of ammonia atmosphere, after reaction with anhydrous
Ethyl alcohol washs 2~3 times, takes off film after being placed in drying box dry 3~5h, then film layer is immersed in Ludox, ammonium hydroxide tune is used in combination
PH to 9~10 is saved, 3~5h is stirred with 400~500r/min, takes out after film layer washs 2~3 times with absolute ethyl alcohol and uses deionized water
Washing 2~3 times, then be placed in drying box and dry to constant weight, obtain super hydrophilic oleophobic type film base water-oil separating material.
Natural air drying after black carp scales are washed with deionized 2 times, then fish scale is spliced into plate, it is used in combination 502 glue to bond
Molding, obtains template base material, and 8g ethyl orthosilicates, 1.0g hexadecane trimethoxy silanes is taken to be added in 100g isopropanols, with
300r/min stirs 20min, then 2g mass fractions are added dropwise as 20% hydrochloric acid with 0.1g/min, continues to stir 20min, obtains Ludox,
2g chitosans are taken, 200g mass fractions are added in 2% acetum, to stir to chitosan and being completely dissolved with 300r/min, then with
4g butyl titanates are added dropwise in 0.3g/min, continue to stir 20min, obtain coating liquid, and coating liquid, control are coated on template base material surface
Film amount is 60g/m2, it is placed in hydrothermal reaction kettle, 10h is reacted under 120 DEG C of ammonia atmosphere, after reaction with anhydrous second
Alcohol washs 2 times, takes off film after being placed in drying box dry 3h, then film layer is immersed in Ludox, ammonium hydroxide is used in combination to adjust pH to 9,
3h is stirred with 400r/min, takes out after film layer washs 2 times with absolute ethyl alcohol and is washed with deionized 2 times, then be placed in drying box
Drying obtains super hydrophilic oleophobic type film base water-oil separating material to constant weight.
Natural air drying after black carp scales are washed with deionized 2 times, then fish scale is spliced into plate, it is used in combination 502 glue to bond
Molding, obtains template base material, and 10g ethyl orthosilicates, 1.2g hexadecane trimethoxy silanes is taken to be added in 120g isopropanols, with
320r/min stirs 25min, then 2g mass fractions are added dropwise as 20% hydrochloric acid with 0.1g/min, continues to stir 25min, obtains Ludox,
2g chitosans are taken, 240g mass fractions are added in 2% acetum, to stir to chitosan and being completely dissolved with 360r/min, then with
5g butyl titanates are added dropwise in 0.4g/min, continue to stir 25min, obtain coating liquid, and coating liquid, control are coated on template base material surface
Film amount is 70g/m2, it is placed in hydrothermal reaction kettle, 11h is reacted under 150 DEG C of ammonia atmosphere, after reaction with anhydrous second
Alcohol washs 2 times, takes off film after being placed in drying box dry 4h, then film layer is immersed in Ludox, ammonium hydroxide is used in combination to adjust pH to 9,
4h is stirred with 450r/min, takes out after film layer washs 2 times with absolute ethyl alcohol and is washed with deionized 2 times, then be placed in drying box
Drying obtains super hydrophilic oleophobic type film base water-oil separating material to constant weight.
Natural air drying after black carp scales are washed with deionized 3 times, then fish scale is spliced into plate, it is used in combination 502 glue to bond
Molding, obtains template base material, and 12g ethyl orthosilicates, 1.5g hexadecane trimethoxy silanes is taken to be added in 150g isopropanols, with
400r/min stirs 30min, then 3g mass fractions are added dropwise as 20% hydrochloric acid with 0.2g/min, continues to stir 30min, obtains Ludox,
3g chitosans are taken, 300g mass fractions are added in 2% acetum, to stir to chitosan and being completely dissolved with 400r/min, then with
6g butyl titanates are added dropwise in 0.5g/min, continue to stir 30min, obtain coating liquid, and coating liquid, control are coated on template base material surface
Film amount is 80g/m2, it is placed in hydrothermal reaction kettle, 12h is reacted under 160 DEG C of ammonia atmosphere, after reaction with anhydrous second
Alcohol washs 3 times, takes off film after being placed in drying box dry 5h, then film layer is immersed in Ludox, ammonium hydroxide is used in combination to adjust pH to 10,
5h is stirred with 500r/min, takes out after film layer washs 3 times with absolute ethyl alcohol and is washed with deionized 3 times, then be placed in drying box
Drying obtains super hydrophilic oleophobic type film base water-oil separating material to constant weight.
The water-oil separating of super hydrophilic oleophobic type film base water-oil separating material prepared by the present invention and the production of Guangdong company
Material is detected；
The functional group of sample surfaces is analyzed using Fourier transform infrared spectroscopy instrument, test environment is room temperature, and data are adopted
Collect ranging from 400 ~ 4000cm-1, data acquisition intervals 1cm-1；
Contact angle test is carried out to obtained sample using optical video contact angle instrument, the special wetting property of sample is characterized, makes
It is test liquid with the deionized water or dimethicone that volume is 3 μ L, record test droplets and sample are stable from touching
Overall process obtains the contact angle values of sample by Instrumental Analysis, and each test sample takes 5 different zones as test point, takes
Average value is contact angle final testing result；
Between separation material is clipped in two glass devices, a diameter of 50mm.Oil water mixture is poured into from top, by wetting
Property and gravity effect, the water in oil water mixture is efficiently separated out, realize water-oil separating.For separation material, divide
It is higher from efficiency, it was demonstrated that the oil-water selectivity of separation material is better, and define water-oil separating test efficiency eta=m1/m2 ×
100%, wherein：M1 is the quality for the water isolated, g；M2 is the quality of water before separation.
Specific testing result such as following table table 1：
1 super hydrophilic oleophobic type film base water-oil separating material property of table characterizes
The super hydrophilic oleophobic type film base water-oil separating material that as shown in Table 1 prepared by the present invention has good underwater hydrophilic and oleophobic property
Can, it is good to can be used for water-oil separating durability, and oily contact angle can reach 158 ° or more, and the present invention's is simple for process, can criticize
Amount generates, at low cost, use easy to spread.
Claims (6)
1. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material, which is characterized in that specifically preparation process is：
（1）Natural air drying after black carp scales are washed with deionized 2~3 times, then it is used in combination 502 glue viscous at plate fish scale linking
Form type, obtains template base material；
（2）Ethyl orthosilicate, hexadecane trimethoxy silane is taken to be added in isopropanol and be uniformly mixed, then mass fraction is added dropwise and is
20% hydrochloric acid stirs 20~30min, obtains Ludox；
（3）It is that stirring to chitosan is completely dissolved in 2% acetum, then four fourth of metatitanic acid is added dropwise to take chitosan that mass fraction is added
Ester stirs 20~30min, obtains coating liquid；
（4）Coating liquid is coated on template base material surface, is placed in hydro-thermal process in hydrothermal reaction kettle, alcohol washes drying after reaction
And film is taken off, then film layer is immersed in Ludox and is stirred to react 3~5h, drying after film layer is washed with alcohol wash water successively is taken out, is obtained super
Hydrophilic and oleophobic type film base water-oil separating material.
2. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material as described in claim 1, which is characterized in that
Step（2）The ethyl orthosilicate, hexadecane trimethoxy silane, isopropanol, hydrochloric acid parts by weight be 8~12 parts of positive silicic acid second
Ester, 1.0~1.5 parts of hexadecane trimethoxy silanes, 100~150 parts of isopropanols, 2~3 parts of hydrochloric acid.
3. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material as described in claim 1, which is characterized in that
Step（3）The chitosan, acetum, butyl titanate parts by weight be 2~3 parts of chitosans, 200~300 parts of acetic acid are molten
Liquid, 4~6 parts of butyl titanates.
4. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material as described in claim 1, which is characterized in that
Step（4）The film amount of the coating liquid is 60~80g/m2.
5. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material as described in claim 1, which is characterized in that
Step（4）The hydrothermal treatment process is that 10~12h is reacted under 120~160 DEG C of ammonia atmosphere.
6. a kind of preparation method of super hydrophilic oleophobic type film base water-oil separating material as described in claim 1, which is characterized in that
Step（4）It is described to be stirred to react to adjust pH to 9~10 with ammonium hydroxide and stirring 3~5h with 400~500r/min.
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Cited By (3)
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| CN109603579A (en) * | 2018-12-03 | 2019-04-12 | 宁波大学 | A kind of preparation method and applications of chitin-tetraethyl orthosilicate composite membrane |
| CN111672334A (en) * | 2020-06-18 | 2020-09-18 | 上海恩捷新材料科技有限公司 | Dual hydrophilic polyethylene ultrafiltration membrane and preparation method thereof |
| CN114163180A (en) * | 2022-01-06 | 2022-03-11 | 郭智霖 | Antiskid water permeable brick and preparation method thereof |
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Application publication date: 20180907 |